A novel suite of instrumentation for the characterisation of materials held inside an air-tight tube furnace operated up to 250 °C has been developed. Real-time detection of released gases (volatile organic compounds (VOCs), CO2, NO, NO2, SO2, CO and O2) was achieved combining commercial off-the-shelf (COTS) gas sensors and sorbent tubes for further qualitative and semi-quantitative analysis by gas chromatography-mass spectrometry coupled to thermal desorption (TD-GC-MS). The test system was designed to provide a controlled flow (1000 cm3 min-1) of hydrocarbon free air through the furnace. The furnace temperature ramp was set at a rate of 5 °C min-1 with 10 min dwell points at 70 °C, 150 °C, 200 °C and 250 °C to allow time for stabilisation and further headspace sampling onto sorbent tubes. Experimental design of the instrumentation is described here and an example data set upon exposure to a gas sample is presented.